EP1582101B1 - Procédé de fabrication d'un complément alimentaire pour animaux de forme granulaire et contenant de la L-lysine - Google Patents

Procédé de fabrication d'un complément alimentaire pour animaux de forme granulaire et contenant de la L-lysine Download PDF

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Publication number
EP1582101B1
EP1582101B1 EP05356057A EP05356057A EP1582101B1 EP 1582101 B1 EP1582101 B1 EP 1582101B1 EP 05356057 A EP05356057 A EP 05356057A EP 05356057 A EP05356057 A EP 05356057A EP 1582101 B1 EP1582101 B1 EP 1582101B1
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EP
European Patent Office
Prior art keywords
lysine
content
granules
concentrate
granulator
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Revoked
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EP05356057A
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German (de)
English (en)
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EP1582101A1 (fr
Inventor
Soon Won Hong
Gyu Nam Cho
Yong Bum Seo
Seung Woo Han
Jae Hun Yu
Hyun Tae Kim
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CJ CheilJedang Corp
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CJ CheilJedang Corp
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Classifications

    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K10/00—Animal feeding-stuffs
    • A23K10/10—Animal feeding-stuffs obtained by microbiological or biochemical processes
    • A23K10/16—Addition of microorganisms or extracts thereof, e.g. single-cell proteins, to feeding-stuff compositions
    • A23K10/18—Addition of microorganisms or extracts thereof, e.g. single-cell proteins, to feeding-stuff compositions of live microorganisms
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K10/00—Animal feeding-stuffs
    • A23K10/10—Animal feeding-stuffs obtained by microbiological or biochemical processes
    • A23K10/12—Animal feeding-stuffs obtained by microbiological or biochemical processes by fermentation of natural products, e.g. of vegetable material, animal waste material or biomass
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/10—Organic substances
    • A23K20/142—Amino acids; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K40/00—Shaping or working-up of animal feeding-stuffs
    • A23K40/10—Shaping or working-up of animal feeding-stuffs by agglomeration; by granulation, e.g. making powders
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K40/00—Shaping or working-up of animal feeding-stuffs
    • A23K40/30—Shaping or working-up of animal feeding-stuffs by encapsulating; by coating
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S426/00—Food or edible material: processes, compositions, and products
    • Y10S426/807—Poultry or ruminant feed

Definitions

  • the present invention relates to a method for preparing lysine granules used as an animal feed additive and lysine granules prepared by the method.
  • U.S. Patent No. 5,431,933 discloses an animal feed additive containing most of components of a fermentation broth and a method for preparing the same. According to the method disclosed in this patent, a slightly hygroscopic and sticky animal feed additive with an amino acid content of 40 to 90% can be prepared at a low cost.
  • the animal feed additive has disadvantages such as a low density and a large variation in component contents. That is, the content of a lysine in the fermentation broth varies according to a fermentation condition, which in turn causes a variation in the content of a lysine contained in the animal feed additive based on the fermentation broth.
  • U.S. Patent No. 5,622,710 discloses a method for preparing animal feed additive pellets, which includes: directly spray-drying a fermentation broth containing an assimilable sugar of 0.3% or less to obtain fine granules and mixing the fine granules with a binder such as water and a fermentation broth.
  • the animal feed additive pellets prepared according to this method disclosed in this patent have a density of 550 kg/m' or more, an amino acid content of 40 to 90%, and low hygroscopic property and stickiness.
  • the formation of the fine granules from the fermentation broth and the mixing of the fine granules with the fermentation broth by an intensive mixer increase a process complexity.
  • U.S. Patent No. 5,133,976 discloses a method for preparing an animal feed additive containing a lysine content of 35 to 48%, which includes: culturing a lysine producing microorganism while maintaining an assimilable sugar of 5 to 15 g/l; concentrating the resultant culture to obtain a concentrate with a solid content of 50 to 75%; and dehydrating the concentrate by azeotropic distillation.
  • a lysine content is low, the azeotropic distillation increases a process cost and a process complexity, and the animal feed additive is easily made into fine powders.
  • EP 923 878 discloses a process for producing an L-lysine feed supplement with an adjustable amount of L-lysine purity in a range between about 35% and 80% L-lysine. A material containing L-lysine is added to a substantially cell free L-lysine broth, then the mixture is dried.
  • EP 467 401 discloses a feed additive granule for ruminants comprising a granulated physiologically active substance as a core, and first and second coating layers having protecting ability with respect to pH values.
  • the present invention provides a method for efficiently preparing a granular animal feed additive while maintaining the content of a lysine constant.
  • the present invention also provides a granular animal feed additive having a standardized lysine content prepared by the method.
  • a method for preparing a granular animal feed additive which comprises: filtering, with a membrane filter, a fermentation broth obtained from a lysine producing microorganism cultured in a lysine producing condition to obtain a lysine-containing filtrate and a microorganism-containing sludge; drying the filtrate to obtain a concentrate with a total solid content of 48 to 52 wt%; granule-drying the concentrate at a temperature of 50°C to 60°C to obtain granules; and coating the granules with a coating agent containing one or more selected from the group consisting of the sludge, a diluent or a free lysine as a
  • a granular animal feed additive prepared by the method.
  • the present invention provides a method for preparing a granular animal feed additive, which includes: filtering, with a membrane filter, a fermentation broth obtained from a lysine producing microorganism cultured in a lysine producing condition to obtain a lysine-containing filtrate and a microorganism-containing sludge; drying the filtrate to obtain a concentrate with a total solid content of 48 to 52 wt%; granule-drying the concentrate at a temperature of 50°C to 60°C to obtain granules; and coating the granules with a coating agent containing one or more seiected from the group consisting of the sludge, a diluent or a free lysine as a lysine content adjustor, and a moisture prevention agent, to obtain lysine granules having the following properties: Lysine content (lysine sulfate) 65% or more Grain size 300-1,200 ⁇ m, 90% or more Apparent density
  • the granules are preferably obtained by spraying the concentrate into a granulator from the bottom of the granulator and applying a hot air to the concentrate in the granulator to form a fluidized bed.
  • a common fluidized bed granulator may be used.
  • the granulation can be performed in an appropriate operating condition.
  • the flow rate of the concentrate, a nozzle pressure, and the air volume during the granulation may be adjusted so that 90% or more of the granules have a grain size of 300 to 1,200 ⁇ m.
  • the diluent is one or more selected from the group consisting of starch, carageenan, and agar.
  • the moisture prevention agent includes a polymer, preferably liquid paraffin.
  • the microorganism that can be used herein provided that it can produce a lysine.
  • a strain of Corynebacterium sp. that is often used in lysine fermentation is preferable.
  • the fermentation condition for the lysine producing microorganism is not particularly limited, it is preferable to culture the lysine producing microorganism in a condition such that a large amount of lysine and a small amount of biomass are accumulated. Since sugar contained in the fermentation broth prevents the drying of the fermentation broth and increases the hydroscopic property of the lysine granules, it is preferable to set the fermentation condition toward reduction of a sugar content. In the present invention, however, since the lysine content and the hydroscopic property can be controlled by the coating process, there is no need to limit the fermentation condition to the above-described condition.
  • the fermentation broth is filtered by membrane filtration.
  • the fermentation broth is separated into the filtrate and the sludge by the filtration.
  • the sludge contains components for animal nutrition and is reused in the subsequent coating process.
  • the membrane filter that can be used herein provided that it can separate the microorganism from the fermentation broth.
  • One of ordinary persons skilled in the art might easily set the operating condition of the membrane filter to separate the microorganism from the fermentation broth. For example, the fermentation broth that has been previously heated at about 60°C is pressed toward the membrane filter for about 1 hour to form a gel layer. Then, the filtration is carried out in a condition that the temperature of the fermentation broth is about 60°C and a transmembrane pressure (TMP) is 1.2 to 1.5 atm. It is understood that one of ordinary persons skilled in the art can easily select a pore size of the membrane filter.
  • TMP transmembrane pressure
  • the filtrate obtained by the membrane filtration is dried to have a solid content of 48 to 52%.
  • the drying process serves to reduce the total volume of the filtrate with relatively increasing lysine content by decreasing the water content of the filtrate.
  • the drying process is well known in the art. A reduced-pressure drying may be used.
  • the concentrate obtained by the drying is granulated to form the granules.
  • the concentrate is heated at a temperature of 50°C to 60°C for the granulation.
  • the viscosity of the concentrate decreases, which is helpful in uniform mixing of the concentrate without lumping and formation of uniform granules. If the granulation temperature exceeds 60°C, costs for the granulation is economically too high. On the other hand, if it is less than 50 °C, reduction of viscosity may be insignificant, thereby making difficult to form a granule and decreasing the bulk density of the resultant granule and increasing the hygroscoposity of the resultant granule.
  • a hot air is continuously supplied so that predetermined sized particles formed by the spraying form a fluidized bed.
  • a common fluidized bed granulator may be used.
  • the granulation may be carried in the following non-limiting conditions: a heater temperature of 170°C, an inlet temperature of 140 to 160°C, an outlet temperature of 60 to 70°C, and a spraying pressure of 1.8 to 2.0 bar.
  • the granules obtained by the granulation may be further subjected to a sieving process. Desired sized granules are transferred to a subsequent process. Under-sized granules may be returned to the granulation and over-sized granules may be pulverized and then returned to the granulation.
  • the granules obtained by the granulation or the sieving are subjected to the coating process.
  • the coating process is well known in one of ordinary persons skilled in animal feed or drug related industries. Any coater may be used during the coating process.
  • a commercially available coater may be used.
  • a material that can be used for the coating process is the coating agent containing one or more selected from the group consisting of the sludge obtained by the filtration, a diluent or a free lysine as a lysine content adjustor, and a moisture prevention agent.
  • the sludge is used for utilizing useful substances contained in the microorganism.
  • the lysine content adjustor is used to adjust the content of lysine in the granules.
  • the lysine content adjustor is optionally used according to the content of lysine. That is, when the content of lysine exceeds a predetermined value, the coating agent containing the diluent is coated on the granules to decrease the content of lysine. On the other hand, when the content of lysine is less than a predetermined value, the coating agent containing the free lysine is coated on the granules to increase the content of lysine. Therefore, the lysine content of the granules obtained by the present invention can be adjusted within an error range of about 1%.
  • the moisture prevention agent serves to decrease the hygroscopic property of the lysine granules, which enables long-term storage.
  • the lysine granules obtained according to a method of the present invention have the following characteristics: the content of lysine (based on lysine sulfate) is 65% or more in dry mass, a grain size of 300-1,200 ⁇ m is 90% or more, an apparent density is 620-720 kg/m 3 , a protein content is 10-15%, a total sugar content is >0-1 %, an inorganic material content is >0-3%, a water content is >0-3%, a C 8 or less carboxylic acid content is >0-8%, and a SO 4 - ion content is 20-25%.
  • Example 1 Fermentation, filtration, concentration, and granulation
  • Corynebacterium glutamicum CJM107 (KCCM-10227) was cultured in 18 liters of a culture medium containing 50g of raw sugar, 10g of peptone, 10g of Yeast Extract, 5g of urea, 4g of KH 2 PO 4 , 8g of K 2 HPO 4 , 0.5g of MgSO 4 ⁇ 7H 2 O, 100 ⁇ g of biotin, 1,000 ⁇ g of thiamine HCI for 96 hours at 35 °C, pH 6-8 to obtain a fermentation broth.
  • the fermentation broth contained a lysine of 15.1 %.
  • the fermentation broth recovered was heated at 60°C and filtered using a membrane filter (Ceramic Filter Pilot : pore size 0.05 ⁇ m, area 4.7 m 2 ) in a transmemebrane pressure (TMP) of 1.2-1.5 atm to separate a microorganism sludge and a filtrate.
  • the filtrate thus obtained has a lysine content of 18.7% and a total solid of 25.8%.
  • the filtrate was dried under a reduced pressure of a vacuum of 680 mmHg and at a temperature of 65°C to obtain a concentrate with a lysine content of 37.1% and a total solid of 51.2% and then the reaction temperature was reduced to 60°C.
  • the concentrate was granulated with a granulator (GR Engineering, Fluid Bed Spray Dryer).
  • a granulator GR Engineering, Fluid Bed Spray Dryer
  • the concentrate was supplied into the granulator by a bottom spray method through a lower nozzle of the granulator.
  • the granulator was operated in the following conditions: a heater temperature of 170°C, an inlet temperature of 140-160°C, an outlet temperature of 60-70°C, and a spray pressure of 1.8-2.0 bar.
  • the concentrate supplied into the granulator was solidified by hot air drying.
  • the solidified concentrate was subjected to crashing and agglomeration with a freshly supplied concentrate to form larger granules while flowing in a fluidized bed.
  • the granules obtained in this Example had a lysine content of 69.4%, a water content of 0.04%, an inorganic material content of 2.53%, and an apparent density of 635.2 kg/m'.
  • Example 2 Preparation of lysine granules coated with coating agent containing diluent
  • Fermentation, filtration, concentration by evaporation of a filtrate, and granulation of a concentrate were performed in the same manner as in Example 1.
  • the filtrate had a lysine content of 13.97% and a total solid of 22.8%.
  • the concentrate obtained by evaporation of the filtrate under a reduced pressure had a lysine content of 41.5%, a total solid of 50.5%, a volume and a specific gravity of 20 L and 1.150, respectively.
  • the granules obtained by fluidized-bed drying of the concentrate had a lysine content of 69.2%, a water content of 0.12%, an inorganic material content of 2.53%, and a total weight of 4.1 kg.
  • the granules thus obtained were coated with an aqueous diluent solution (water content of 9.3%) obtained by dissolving 0.25 kg of a diluent (corn starch) in water (0.5 L) as a coating agent.
  • granules had a lysine content of 65.7%, a water content of 0.14%, protein content 0.36%, total sugar 0.8%, inorganic material 2.6%, carboxylic acid less than Carbon number 8 7.6% and sulfate ion 22.8 %.
  • the bulk density and the weight of the resultant granules were 634.5 kg/m' and 4.3 kg, respectively.
  • Example 3 Preparation of granules coated with coating agent containing microorganism sludge and lysine content adjustor
  • Fermentation, filtration, evaporative concentration, and granulation were performed in the same manner as in Example 1 except that the granules were coated with a coating agent containing a microorganism sludge obtained by the filtration and a free lysine.
  • the fermentation broth was obtained in an amount of 30.0 L and had a lysine content of 15.5%.
  • the filtrate had a lysine content of 18.7% and a total solid of 25.8%.
  • the concentrate obtained by evaporation of the filtrate under a reduced pressure had a lysine content of 30.2%, a total solid of 50.3%, a water content 49.7 %, a volume and a specific gravity of 15.4 L and 1.210, respectively.
  • the granules obtained by fluidized-bed drying of the concentrate had a lysine content of 68.9%, a water content of 0.26%, an inorganic material content of 2.29%, and a density of 650.3 kg/m 3 , and a total weight of 1.06 kg.
  • the granules thus obtained were coated with a mixture obtained by dissolving 0.2kg of the solid of the microorganism sludge obtained by the filtration, and 123 g of a 99% free lysine (to adjust the total lysine content of finally obtained granules to 65% including the consideration of the lysine content of the microorganism sludge and the like) in water.
  • the finally obtained granules had a lysine content of 65.4%, a protein content 2.25%, total sugar content 1.05%, carboxylic acid having less 8 carbon number 7.6%, a water content of 0.23%, an inorganic material content of 2.67% and sulfate ion content 20.8%.
  • the bulk density and the weight of the resultant granules were 642.6 kg/m 3 and 1.65 kg. 91.3% of the granules had a grain size of 300-1,200 ⁇ m.
  • lysine granules with a lysine content within an error range of about 1% and significantly low sugar content can be obtained. Therefore, when the lysine granules are used as an animal feed additive, they can be stored for a long-term due to a low hygroscopic property and the usage amount of the lysine granules can be precisely adjusted.

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Zoology (AREA)
  • Food Science & Technology (AREA)
  • Animal Husbandry (AREA)
  • Biotechnology (AREA)
  • Microbiology (AREA)
  • Proteomics, Peptides & Aminoacids (AREA)
  • Health & Medical Sciences (AREA)
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  • Preparation Of Compounds By Using Micro-Organisms (AREA)

Claims (7)

  1. Procédé de préparation d'un additif alimentaire pour animaux de forme granulaire, qui comprend :
    la filtration, avec un filtre à membrane, d'un bouillon de fermentation obtenu à partir d'un microorganisme produisant de la lysine cultivé dans des conditions permettant la production de lysine afin d'obtenir un filtrat contenant de la lysine et une boue contenant des microorganismes ;
    le séchage du filtrat pour obtenir un concentré présentant une teneur en solide totale de 48 à 52 % en poids ;
    le séchage par granulation du concentré à une température comprise entre 50 °C et 60 °C pour obtenir des granules ; et
    l'enrobage des granules avec un agent d'enrobage contenant un ou plusieurs éléments choisis dans le groupe constitué par la boue, un diluant ou une lysine libre en tant qu'agent d'ajustement de la teneur en lysine et un agent de protection contre l'humidité, pour obtenir des granules de lysine présentant les propriétés suivantes : Teneur en lysine (sulfate de lysine) 65 % ou plus Taille de grain 300 à 1 200 µm, 90 % ou plus Densité apparente 620 à 720 kg/m2 Teneur en protéines 10 à 15 % Teneur en sucre totale > 0 à 1 % Teneur en matières inorganiques > 0 à 3 % Teneur en eau > 0 à 3 % Teneur en acide carboxylique > 0 à 8 % Teneur en ions SO4 20 à 25 %
  2. Procédé selon la revendication 1, dans lequel lors de la granulation, les granules sont formés par pulvérisation du concentré dans un granulateur à partir de la base du granulateur et l'application d'air chaud au concentré dans le granulateur.
  3. Procédé selon la revendication 1, dans lequel au cours de la granulation, le débit du concentré, la pression de buse et le volume d'air sont ajustés de sorte que 90 % ou plus des granules présentent une taille de grain de 300 à 1 200 µm.
  4. Procédé selon la revendication 1, dans lequel le diluant est composé d'un ou plusieurs éléments choisis dans le groupe constitué par l'amidon, le carraghénane et l'agar-agar.
  5. Procédé selon la revendication 1, dans lequel l'agent de protection contre l'humidité est une paraffine liquide.
  6. Procédé selon la revendication 1, dans lequel le microorganisme produisant de la lysine est une souche de Corynebacterium sp.
  7. Additif alimentaire pour animaux sous forme granulaire susceptible d'être obtenu par le procédé selon l'une quelconque des revendications 1 à 6.
EP05356057A 2004-04-02 2005-03-31 Procédé de fabrication d'un complément alimentaire pour animaux de forme granulaire et contenant de la L-lysine Revoked EP1582101B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR1020040022888A KR101052573B1 (ko) 2004-04-02 2004-04-02 균일한 함량을 갖는 과립형 동물 사료 첨가제를 제조하는 방법 및 그에 의하여 제조되는 과립형 동물 사료 첨가제
KR2004022888 2004-04-02

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EP1582101A1 EP1582101A1 (fr) 2005-10-05
EP1582101B1 true EP1582101B1 (fr) 2009-01-07

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EP05356057A Revoked EP1582101B1 (fr) 2004-04-02 2005-03-31 Procédé de fabrication d'un complément alimentaire pour animaux de forme granulaire et contenant de la L-lysine

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Country Link
US (1) US7514111B2 (fr)
EP (1) EP1582101B1 (fr)
KR (1) KR101052573B1 (fr)
CN (1) CN1676018B (fr)
DE (1) DE602005012170D1 (fr)
DK (1) DK1582101T3 (fr)
WO (1) WO2006004292A1 (fr)

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DE102008001874A1 (de) 2008-05-20 2009-11-26 Evonik Degussa Gmbh Verfahren zur Herstellung von L-Aminosäuren
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DE102009030342A1 (de) 2009-06-25 2010-12-30 Evonik Degussa Gmbh Verfahren zur fermentativen Herstellung von organisch chemischen Verbindungen
CN102191288B (zh) * 2011-03-18 2012-08-15 宁夏伊品生物科技股份有限公司 赖氨酸的反式发酵制备
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DE102011006716A1 (de) 2011-04-04 2012-10-04 Evonik Degussa Gmbh Mikroorganismus und Verfahren zur fermentativen Herstellung einer organisch-chemischen Verbindung
DE102011118019A1 (de) 2011-06-28 2013-01-03 Evonik Degussa Gmbh Varianten des Promotors des für die Glyzerinaldehyd-3-phosphat-Dehydrogenase kodierenden gap-Gens
JP5967982B2 (ja) 2012-03-07 2016-08-10 東レエンジニアリング株式会社 プラズマｃｖｄ法により形成された化学蒸着膜
CN103451221B (zh) * 2012-11-07 2016-05-04 宁夏伊品生物科技股份有限公司 发酵制备高纯度赖氨酸盐的方法及其产品
CN103805646B (zh) * 2012-11-07 2015-09-30 宁夏伊品生物科技股份有限公司 发酵制备高纯度赖氨酸盐的方法及其产品
CN102925506B (zh) * 2012-11-07 2013-10-16 宁夏伊品生物科技股份有限公司 发酵制备高纯度赖氨酸硫酸盐的方法
EP2762571A1 (fr) 2013-01-30 2014-08-06 Evonik Industries AG Microorganisme et procédé de fabrication par fermentation d'acides aminés
EP2932856B1 (fr) 2014-04-07 2017-08-23 Evonik Degussa GmbH Procédé de granulation en lit fluidisé de bouillons de fermentation contenant des acides aminés
EP2940144A1 (fr) 2014-04-30 2015-11-04 Evonik Degussa GmbH Procédé de production de L-lysine en utilisant une bactérie alcaliphile
WO2018202686A1 (fr) 2017-05-03 2018-11-08 Nestec S.A. Base d'arôme naturel et procédé pour sa préparation
WO2019182413A1 (fr) * 2018-03-23 2019-09-26 씨제이제일제당 (주) Granules contenant de l'acide l-aminé et leur procédé de préparation
CN109321434A (zh) * 2018-12-05 2019-02-12 江苏澳创生物科技有限公司 一种色氨酸饲料添加剂生产系统
TW202333581A (zh) * 2021-12-24 2023-09-01 南韓商Ｃｊ第一製糖股份有限公司 由發酵液製備含胺基酸製品之方法
WO2024215042A1 (fr) * 2023-04-13 2024-10-17 씨제이제일제당 (주) Granulé de lysine à structure cœur-écorce

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8802400B2 (en) 2005-10-08 2014-08-12 Evonik Degussa Gmbh L-lysine-containing feed additives
US9023347B2 (en) 2005-10-08 2015-05-05 Evonik Degussa Gmbh L-lysine containing feed additives

Also Published As

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DE602005012170D1 (de) 2009-02-26
CN1676018A (zh) 2005-10-05
CN1676018B (zh) 2010-05-05
US7514111B2 (en) 2009-04-07
WO2006004292A1 (fr) 2006-01-12
KR20050097678A (ko) 2005-10-10
EP1582101A1 (fr) 2005-10-05
KR101052573B1 (ko) 2011-07-29
US20050220933A1 (en) 2005-10-06
DK1582101T3 (da) 2009-03-09

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